A neutron polarization analysis study of Ce2Fe17 in its paramagnetic phase

Spin-flip (paramagnetic) scattering and neutron depolarization studies were performed on Ce₂Fe₁₇ in its paramagnetic phase on the Dhruva neutron polarization analysis spectrometer. The absence of normalQ dependence of the scattered spin flip intensity shows that Ce₂Fe₁₇ is not a normal paramagnetic and there exist superparamagnetic clusters of sufficiently large dimensions (～100Å). The observed neutron depolarization gives an indication of the dynamics of these Ce₂Fe₁₇ superparamagnetic clusters.     

The influence of synthetic conditions on the stability of methotrexate-monoclonal antibody conjugates determined by reversed phase high performance liquid chromatography.

Methotrexate (MTX) has been convalently attached to an IgG-type monoclonal antibody (791T/36) directed to tumour-associated antigen gp72. Conjugates were synthesized by the active ester method using MTX N-succinimidyl ester at various pH values (7.5-10.5). Following purification by gel filtration, high performance liquid chromatography was used to assess the free drug or its derivatives in samples of MTX-791T/36 conjugates previously treated (or not) with hydroxylamine. Quantitative analysis, performed on a reversed phase column (pore size 300 A) with isocratic acetonitrile-sodium acetate buffer (pH 4.8) as mobile phase, indicated no detectable amount of free methotrexate in hydroxylamine-treated conjugates even six months after their preparation. Similar observations were made with conjugates, whose synthesis were performed at pH greater than or equal to 10. In contrast, the presence of increasing amounts of drug/metabolite could be demonstrated in samples produced at lower pH values. Based on these findings, the pH-dependent kinetics of MTX release has been determined and used to design conditions under which stable MTX-791T/36 conjugates could be prepared without hydroxylamine reaction.     

Novel monohydrogenphosphate sensor based on vanadyl salophen

A novel PVC-based membrane sensor based on vanadyl salophen (VNSP) for determination of trace amounts of monohydrogenphosphate (MHP) ions is introduced. The electrode revealed Nernstian response towards monohydrogenphosphate over the wide concentration range from 1.0×10⁻¹ to 1.0×10⁻⁶ M at the pH of 8.2. The effect of solvent mediator, cationic additives and amount of ion-carrier on the behavior of the sensor was investigated. The sensor shows a short response time (<20 s) in the whole concentration ranges. The selectivity of the electrode is very high, and it can be used for detection of trace amounts of monohydrogenphosphate in the presence of large amounts of other anions. The detection limit of the electrode was 5.0×10⁻⁷ M (48 ng/ml) and it could be used for 14 weeks without any measurable changes in the slope. The potentiometric selectivity coefficients data revealed negligible interference from 16 common anions. It was successfully applied for the direct determination of monohydrogenphosphate in fertilizer samples and, as an indicator electrode, in potentiometric titration of HPO₄²⁻ ion with barium nitrate.     

Trichloroisocyanuric acid as a novel oxidizing agent for the oxidation of 1,3,5-trisubstituted pyrazolines under both heterogeneous and solvent free conditions

Trichloroisocyanuric acid is used as an effective oxidizing agent for the oxidation of 1,3,5-trisubstituted pyrazolines to their corresponding pyrazoles under both heterogeneous and also solvent free conditions with good yields at room temperature.     

Solid-liquid extraction and preconcentration of trace nickel using 2-nitroso-1-naphthol-4-sulfonic acid (Nitroso-S) and TDBA onto benzophenone and determination by atomic absorption spectrometry.

Nickel was quantitatively retained by 2-nitroso-1-naphthol-4-sulfonic acid (Nitroso-S) and tetradecyldimethylbenzylammonium chloride (TDBA Cl) onto benzophenone in the pH range 5.0-6.0 from large volumes of aqueous solutions of various samples. After filtration, each solid mass consisting of a nickel complex and benzophenone was dissolved with 5 ml of dimethylformamide (DMF) and the metal was determined by atomic absorption spectrometry (AAS). About 0.6 microg of nickel could be concentrated from 200 ml of an aqueous sample, where its concentration was as low as 3.0 ng/ml. Eight replicate determinations of 2.5 microg/ml of nickel in the final DMF solution gave a mean absorbance of 0.112 with a relative standard deviation of 1.9%. The sensitivity for 1% absorption was 98 ng/ml. The interference of a number of anions and cations was studied and the developed optimized conditions were utilized for the trace determination of nickel in various alloys and biological samples.     

Isolating the most recent entry in a random recursive tree by random cuts

A recursive tree is constructed by starting with a root node and repeatedly adjoining new nodes to one node of the tree already constructed. Such a tree can represent, for example, the heirarchy of a workforce of a company that grows via recruiting. At times of economic depression, the company may decide to lay off participants, and in some cases it is a fair policy to relieve the last senior worker (most recent entry in the tree). If we remove an edge from such a tree then it falls into two subtrees one of which contains the most recent entry. If we continue to remove edges from the successively smaller subtrees that contain the most recent entry, we eventually isolate the most recent entry. We consider how many randomly selected edges must be removed in average before isolating the most recent entry by this procedure.     

Studies on recoil proton tracks in NTA films with the T(d,n)He reaction

Recoil proton tracks in nuclear emulsion are counted by scanning them using strip, square or circular field of view of optical microscope. In this paper, the overestimate due to the edge effects in counting recoil proton tracks at different neutron energies produced from the T(d,n)⁴He reaction has been determined by measuring the true track density in NTA film. The overestimate has also been calculated using the measured value of the mean projected track length (L) in the film. The percentage of measured overestimates has been compared with those obtained by calculation and the results agree reasonably well. Fading effect in NTA film has been studied and found to be 22% more in the summer than in the winter season. A great reduction in fading rate could be achieved if the films are desiccated and sealed in highly pure dry nitrogen maintained at an over-pressure of 1000 Pa to reduce water vapour ingress. After the edge effect correction, the sensitivity of NTA film has been calculated from (1.72±0.08)×10⁻³ tracksn⁻¹ to (1.97±0.16)×10⁻³ tracksn⁻¹ in the neutron energy ranges from 15.91 to 18.88 MeV. The response was found to be from 0.24±0.02 trackscm⁻² permSv to 0.26±0.01 trackscm⁻² permSv in the same energy range.     

Novel route to synthesis of allyl starch and biodegradable hydrogel by copolymerizing allyl‐modified starch with methacrylic acid and acrylamide

Maize starch was modified by allyl chloride adopting an interfacial reaction technique with cetyltrimethyl ammonium bromide as a phase‐transfer catalyst and pyridine as an acid acceptor. The degree of substitution was determined from an increasing carbon content of the modified starch. The percentage of carbon and hydrogen of the allyl‐modified starch was estimated by elemental analysis (C, H, and N), and the product characterization was done through ¹H NMR and ¹³C NMR analyses. The allyl‐modified starch was then copolymerized with methacrylic acid and a combination of methacrylic acid and acrylamide at 50 and 70 °C with potassium persulfate as an initiator. The copolymer thus formed swelled in distilled water after neutralization with sodium carbonate. The percentage of absorption capacity of the hydrogels was determined with distilled water and 0.9% NaCl solution. The highest percentage of absorption, 6500%, was achieved for the developed hydrogel containing allyl starch and acrylic monomer in a 1.7:1 w/w ratio and acrylic monomer, namely, methacrylic acid and acrylamide in a 3.2:1 w/w ratio. The study on biodegradability of the developed hydrogel showed that the hydrogel is degradable in the presence of diastase (amylase). © 2003 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 41: 1650–1658, 2003